Apparatus for distilling anhydrous ammonia



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J. E. HOLMES. I 4 A APIARATUS FOR DISTILLING ANHYDROUS AMMONIA.

No. 410,244. Patented Sept. 3, 1889.

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'JPE. HOLMES. APPARATUS FOR DISTILLING ANHYDROUS AMMONIA. No. 410,244. A Patented Sept. 3, 1889.

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V J.E.H-OLMES. APPARATUS FOR DISTI-LLING ANHYDROUS AMMONIA.

No. 410,244; 7 A V Patente dSept. s, 1889.

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UNITED STATES PATENT OF ICE,

JOSEPH E. HOLMES, OF \VASHINGTON, DISTRICT OF COLUMBIA, ASSIGNOR TO THE AMERICAN AUTOMATIC REFRIGERATING COMPANY,'OF RICHMOND,

VIRGINIA.

APPARATUS FOR DISTILLING ANHYDROUS AMMONIA.

SPECIFICATION forming part of Letters Patent No. 410,244, dated September 3, 1889.

Application filed December 5,1888. Serial No. 292,702. (No model.) I

To all whom it may concern:

Be it known that I, JOSEPH E. HOLMES, a citizen of the United States, residing at Washington, in the District of Columbia, have invented certain new and useful Improvements in Apparatus for Distilling and Redistilling Ammonia; and I do hereby declare the following to be a full, clear, and exact description of the invention, such as will enable others skilled 1o in the art to which it appertains to make and use the same.

The invention has for its object the distillation or the redistillation of ammonia from water containing it and the preparation of anhydrous liquefied gas in a simple and economical manner; and it consists in the apparatus hereinafter described, and particularly pointed out in the claims.

The following specification, in connection with the accompanying drawings, is sufficiently full and clear to enable those skilled in the art to construct and use said apparatus.

Figure 1 is a plan view; Fig. 2, a sectional side elevation, and Fig. 3 is a transverse section on line a: 0c.

A is a tank set in the brick-work of a furnace over a combustion chamber R, communicating with chimney E This tank and 0 furnace are intended for heating water for the distillation of ammonia contained in water in the stills B and B. The tank is longer and wider than the stills to give a free waterspace around them, and deep enough to allow 5 a perfect immersion of the stills and yet leave a clear space above, as at T in Fig. 3. I preferably shape this tank so that it may conform to the stills, as indicated in the drawin The form shown is strong, presents a large heating-surface, and avoids the use and heat ing of an excess'of water. The stills B B'are placed in this tank, and may be suspended therein by suitable straps of metal from bars resting on the top of .the brick-work, 01' they may rest on light bars beneath them, or may be supported, as shown, by the pipes D and I, passing from the bottoms of the stills through the wall of the tank. The branch pipes I, which communicate with the bottoms of the stills, serve as inlets for filling or outlets for blowing off, stop-cocks Z; and I) being properly manipulated. Pipe D serves to return drip or water of condensation to the still, as will be hereinafter described. From the top of the stills two vapor-pipes extend up- 5 5 wardly and unite in a pipe 0, which is provided with a stop-cock (1. At the other end of the stills two branches rise and unite in pipe P, from which is supported the water-glass P and the pressure-gage 0. Beyond the stop-cock 6o cl extends a pipe C with a slightly-downward inclination, and by a bend returns to the drip-pipe D, with which it connects slightly above the level of the water in the stills, the

length of the.- pipe 0 to this point being about 6 fifty feet or more. Vapors from the stills will be so cooled in these pipes by the surrounding atmosphere that all water, grease, or other foreign impurities will be condensed and deposited in drip-pipe D. From this point, where C connects with the drip -pipe, which is about on a level with the top of the stills, there extends in an upward direction a pipe E, which is a continuation of C. It may be extended in any direction and placed in any desired manner, and located either above or. under ground or in a running stream. The pipe should be extended and have a large 7 capacity by reason of its great length, so that it may hold a large amount of gas and act as a cooler and condenser, and so that the gas shall reach the stop-cock f cooled to the normal temperature under a pressure near to liquefaction, the pressure being produced by the continued distillation of ammonia,

At f, Fig. 1, pipe E is connected with an instrument for transferring gases under pressure, which instrument is fully shown and described in my application for patent filed April 20, 1887, Serial No. 235,515. cated at H, and is composed of two like cylinders, each having one end closed, while the other ends are open and joined by acoupling H which should be well secured and tight.

An elastic sack like diaphragm has its mouth 5 or edge secured at the coupling, while the free end of this sack-like diaphragm is free to move in either direction. The edge of the open end of the sack, provided, if necessary, with a lateral flange or bend, fits between the :00

It is indi- 9o flanges of the coupling, which, when brought together and properly bolted, secure the diaphragm and leave its main body free to be acted upon by any fluid introduced into H through the connecting-pipes G or G.

I show in Fig. 1 asteam-boilerN and pump L, connected with the receptacle H by the pipe K, provided with the stop-cock a, and also connected with the before-described stills by means of the pipe K, having stopcock Z). Stop-cock Z), when open, permits waste water to escape through the pipe J It is not essential that pipes 1 and D should lead from the under side of' the stills, as shown. They may project directly outward from the lower portion of the heads of the stills and pass through the heads of the tank A, the joints being made tight by j am-nuts and asbestus. V

I will nowdescribe the operation'of this apparatus, which is based on certain Well-known characteristics of ammonia. For example, ammonia is readily absorbed by cold water, and also readily escapes from water when it is heated to from about 120 to 190 Fahrenheit. This property, in connection with its great elasticity and the comparative ease with which it can be compressed from a thousand or more volumes to one, enables it to be handled with ease and safety. Premising that the stills, cocks, pipes, and connections described have been thoroughly built in place and tested to at least two hundred and fifty pounds pressure per square inch, the operation is as followsi The tank A is filled with water and stop-cocks a, 1), (1,0, f, and g opened and stop:

cock I) closed. The pump L is then connected through the medium of a suction-pipe M with a tank or holder containing water of ammonia in suflicient quantity to fill the reeeptaele H, and also the two stills B B, up to about the height indicated in Fig. 8, the gageglass P serving as a guide. Before pumping, however, it should be known that the diaphragm occupies that part of H nearestthe pipe K, that air maybe thereby excluded from that end. During the operation of pumping both receptacle H and the stills B B will be filled, and the pump should then be stopped and the cooks a I) closed. Fire is then kindled in the furnace R and the water surrounding the stills heated and also the ammonia-water in the stills. As the heat increases ammonia in the form of gas is expelled through pipes C and E, pushing before it the air in the pipes until traces of gas may be observed passing out of the pipe beyond the open stop-cock g. To prevent waste of the gas,a pipe or hose should then conduct the mingled air and gas into cold water for a little time until all air is expelled. This water can be redistilled. Stop-eoeks f and g are then closed until all ammonia is expelled from the water in the stills, which can be ascertained by opening stop-cock Z) and testingthe water. This op eration being completed and the gas stored in the pipes under pressure, it is shut off from the stills by closing stop-cock d and the drip-pipe cock 6. Blow-off cock 5 may now be opened and the waste water in the stills will be forced out by the elasticity of the gas above its surface. When the stills are thus emptied and cock I) is closed and b and are opened, the water in receptacle H will be forced rapidly into the stills by the gas entering the opposite end of H on the opposite side of the diaphragm therein. The receptacle should be made to hold less than the two stills by twenty or thirty gallons, so that they can never be overfilled. The receptacle H is thus filled'withgas at the same pressure as in the pipes, and the diaphragm is changed to the end near the pump and is ready for a new charge when needed. Stop-cock b is again closed, stop-cocks d and e opened, f is closed, and the distillation renewed. While this distillation proceeds pipe is connected with any strong receptacle for liquefied gas holding any convenient quantity-such as a portable detachable holder for fifty, one hundred, or two hundred pounds or a holder similar to H maybe used and of sufficient capacity to receive five hundred, one thousand, or two thousand pounds for transporting the gas and transferring it to refrigerators or other apparatus for use; or the gas may be forced into mains laid in public streets,which may thus be filled with liquid ammonia-gas. WVhen proper connection is made, the gas in receptacle H (shown in the drawings) is forced into such holder or into mains by opening stop-cock a and stop-cock g andpumpingwalterof ammonia into receptacle H until it is filled and the gas has all left it. When the distillation of a batch is completed, cocks b and b are closed and cock 9 also, and cooks d and c are again opened and the distillation is repeated, and so on while the supply of water of ammonia lasts, or until all cylinders, tanks, or pipes are filled withliquefied gas, or as long as desired. During all these operations the fire need not be drawn, and only heat enough need be maintained to keep the water in the tank A near to the boiling-point, care being taken that the water in the tank shall always be above the stills. As there is no cover to the tan'k, this water can never be heated above the boilingpoint, and the water of ammonia in the still being always under some pressure, very little, if any, watery vapor will pass over through pipe 0, and such as does will be eliminated while passing down the inclined pipe 0 C to the drip D,Whence it Will again mingle with the water in the stills, while the dry gas will pass on and be condensed by the process above described.

I have herein intimated the possibility of carrying liquid ammonia through streetmains, and I shall describe in a separate application for patent novel apparatus for measuring the gas by meter in the expansion-pipes of refrigerators, and also for suspending gasholders on balance frames and seals, and also for connecting the absorbing-tanks with pipes returningito the place or. distillation, so that all transportation of gas or aqua-ammonia in portable vessels is-avoided. As the pumping ure while the distillation is going on, a small ute will be ample for works adapted to pro duce one thousand to two thousand pounds of liquefied gas per day, and the boiler for 1- the pump maybe correspondingly small.

a, I In Fig. 4 is shown a plan View, partlyin section, and in Fig. 5 a transverse section, of a modification of my apparatus adapted to raise coil within the stills B and B, and thence extended outwardly at D and D respectively.

These pipes may be connected in any usual manner to allow the tanks to be filled with water through them, or other well-known devices can be provided for this purpose. Safetyvalves F provide means for regulating the pressure of steam and indirectly controlling the temperature. It is. obvious that such safety-valves might beconnected with each 0 steam-outlet pipe. H II indicate branches of outlet-pipe for ammonia communicating with pipes P and I, as before described with reference to Fig.1.

In operating this apparatus to distill ammonia the larger part of the gas can be expelled at a temperature of about 212 Fahrenheit, or less, free escape of steam from water-tanks being permitted. Toward the end of the distillation a higher temperature, may be desirable, and this can be attained by setting the escape or safety valve to open at a pressure of from one to twenty or more pounds. The described arrangement of the steam-coil has the effect to more quickly heat the interior of the ammonia-water and saves both time and fuel.

In Fig. 6 is shown a diagram or plan View of my stills and transferrer connected with vessels for water wherewith to absorb ammonia-after its use in an ammonia-expanding vessel, (indicated at T.) In this view parts of the tanks and furnace are omitted. The lpump L is shown connected with pipe K and with a return-pipe K. At the opposite end ipes K and K connect with K which by uanches connects with four water vessels or bsorbers k, 10 76 and K0 and a cock zbeing provided in each branch. The expanding vessel T is connected with the several 60 absorbing-vessels by means of the pipe F and its several branches f and four-way coupling f, each branch having a stop-cock f? i In operation,ammonia is introduced into a receiver and into an expanding coil or recep- 6 5 tacle through pipes E and E, a regulator E being interposed between. the receiver and expander. After its expansion the spent am- 5 of the water of ammonia can be done at leispump throwing ten or fifteen gallons per min-..

monia is absorbed through pipe F by water in one of the vessels-as, for example, hip-the cocks being suitably operated. The ammoniated water thus produced can be pumped into the transferrer H and the pressure pro; duced by the pump in the transferrer used to maintain the pressure of ammonia on the opposite side; of the diaphragm therein, this ammoniabeing simultaneously transferred to therefrigerator upon the movement of said absorbing-vessels while the others are being used, as before set forth. These vessels should be provided with small vents to allow the passage of air when a vessel is being filled with or emptied of water, which vents will be closed at proper times to prevent the escape of ammonia. In practice two vessels may be used in any structure to be ref rigerated, one ofwhich is connected to receive compressed. anhydrous ammonia and the other to allow its expansion, an automatic temperatureregulator E being interposed,

substantially as set forth in my patent, No. 357,830, dated February 15, 1887.

It is obvious that more or less than four vessels may be connected with the stills to act as absorbers of ammonia; but the number illustrated is convenient. It is further obvious that the invention may be used either on a small or large scale, the arrangement illustrated in Fig. 6 being suitable for use in a building or block of buildings without the necessity of employing portable holders to con vey anhydrous ammonia from the still to the place of use. It will of course be understood that any number desired of refrigerators or refrigerating-rooms or refrigerating-bnildings can be supplied through pipeE, suitable fixed holders and other devices being placed in each in any well-known manner; and, if desired, pipe E can be made suificiently capacious to IuO IIO

serve as a holder for any desired number of expanding-coils located in refrigerators and each provided with an automatic regulator, in which case independent or separate holders can be dispensed with; and it is further apparent that the length of pipe E, though it should be considerable, would not be objectionable, for the reason that it is desirable that the freshly-distilled ammonia should be cooled as well as condensed before use.

Having thus described my invention and the mode of operating the same, what I claim as new, and desire to secure by Letters Patcut, is-- 1. The combination of the water-tank A, the furnace R, the stills B B, located in the tank, the vapor-eduetion pipe 0, connected to the drip-pipe D, said drip-pipe and inlet-pipe K, provided with stop-cocks b and b, substantially as and for the purpose described.

2. In combination, the transferring-receptacle H, having a movable diaphragm, the pipe K, provided with the stop-cocks a and b, the pipe E, the pump L, and the stills B B, as and for the purposes described.

3. In combination, the transferring-receptacle I-I, the pipe K,vapor-pipe E, provided with the stop-cock f, and suitable tanks, holders, or mains communicating with pipe E by a pipe having stop-cock g, all as and for the purposes described.

4. The combination of a still, a receptacle provided with a flexible diaphragm, pipes connecting the still with the receptacle on each side of the diaphragm, and stop-cocks,whereby the pressure of gas or vapor in the still can at times desired be made to discharge liquid from the receptacle into the still, substantially as and for the purposes described.

5. The combination of a still, a receptacle divided by a sack-like flexible diaphragm, a pipe communicating with the still and also with the receptacle on one side of the diaphragm, a second pipe communicating with the upper part of the still and with the recep tacle on the opposite side of said diaphragm, and stop-cocks and inlets and outlets, substantially as set forth, whereby the still and the receptacle can be filled with ammoniawater and ammonia simultaneously delivered from the other side of the diaphragm, and whereby also ammonia-water can be subsequently expelled from the receptacle and the receptacle simultaneously filled with ammonia on the opposite side of the diaphragm.

G. The combination, with a holder or receptacle for anhydrous ammonia, of stills, a pump,

and a transferrer, as H, the latter being connected with the pump and stills by pipes to receive water from or discharge it into either still, and also to receive ammonia froma still and simultaneously with its reception of water to discharge said ammonia into a holder in a refrigerator or elsewhere without loss of pressure, substantially as specified.

7. The combination, with a holder or receptacle for anhydrous ammonia and with one or more water-vessels connected by pipes having suitable cocks to receive alternately spent ammonia from a vessel for expanding the same, and connected by similar pipes having cocks with stills, of said stills, a pump, and a transferrer, as H, the latter being connected with the pump and stills by pipes to receive water from or discharge it into either still, and also to receive ammonia from a still and simultaneously with its reception of water to discharge said ammonia into a holder in a refrigerator or elsewhere without loss of pressure, substantially as specified.

8. In a distilling apparatus, the combination of a tank or boiler, a still, and a pipe or conduit, the still being located in the water-space of the boiler and the pipe communicating with the steam-space of the boiler and passing through the interior of the still, whereby the latter can be externally heated by water and internally by steam, substantially as set forth.

In testimony whereof I affix my signature in presence of two witnesses.

JOSEPH E. HOLMES.

\Vitnesses:

JOHN T. MITCHELL, BENJ. R. CATLIN. 

